Discussion 'These methods without modification determine 0.1 to 2.5 p.p.m. of 4-dimethylamino-3,5-sylenol, 0.1 to 3.5 p,p.m. of 4-dimethylaiiiino-3~5-xyly1 methylcarbamate, or a total of 0.1 to about 3 p.p.m. of mixtures of the "xylenoi" and the "carbamate" i n peaches and in undelinted cottonseed. The methods for the residue determinations of 4-dimethylamino-3,5xylenol and 4-dimethylamino-3,5-xylyl methylcarbamate in peaches. using water as the water-miscible extraction solvent. should be generally. applicable to the .. analysis of agricultural products with a high water content. The methods for the residue determinations in undelinted cottonseed, using benzene as the Lvaterimmiscible solvent, can be used on agricultural products containing oils and'or little water. Some modifications. of course, may bc necessary.
Table VI. Recovery of Mixtures of 4-Dimethylamino-3,5-xylenol and 4Dimethylamino-3,5-xylyl Methylcarbamate in Undelinted Cottonseed Xylenol Added,
P.P.M. 0.10
0.10 2.00
Corbomate Added,
P.P.M. 0.10
2 00
0 10
Xylenol Found,
Xylenol Recovery,
Carbamate Found,
Carbarnale Recovery,
P.P.M. 0,093
%
P.P.M.
%
0.095 0.105
95 105
0.111 0 105 1 759 1 759
111 105 88 88
0.100
1 914
1 937 0 133 0 133
93 100
96 97
133 133
(5) Pascal, Paul. "Nouveau Traite de Chemie Minerale," Book 14, p. 944, Masson et Cie, Ed., Paris, 1959. (6) Theis, R. C., Benedict, S. R., J. Biol. Chem. 61,67 (1924).
Literature Cited (1) Folin, O.? Ciocoltin, \'., J . Biol. Chem. 73, 627 ( 2 ) Gibbs, H. D., Ibid.,72,649 (1927). (3) Gottlieb, S., Marsh, P. B., Znd. Eng,Chem,,.Anal, Ed, 18, 16 (1946). (4) Lykken, L.. Treseder, R . S . , Zahn, V..Ibid.,18, 103 (1946).
Received for reuierc: July 30, 7962. Accepted .Voormember 13. 1962.
INSECTICIDE RESIDUES IN PROCESSED F O O D S
C. A. ANDERSON and D. MacDOUGALL Chemagro Corp., Kansas City, Mo.
The Effect of Processing on Guthion Residues in Oranges and Orange Products
I
J. W. KESTERSON, R. HENDRICKSON, and R. F. BROOKS Citrus Experiment Station, l a k e Alfred, Fla.
The use of Guthion on citrus necessitated a study of the distribution of residues in citrus byproducts. A study was conducted on Guthion-treated oranges. It was found that standard washing procedure will remove 30% of Guthion residues from treated oranges. The remaining residue is entirely in the peel. Approximately 75% of the residue is destroyed during the treatment involved in production of citrus cattle feed.
G
(trademark.Farbenfabriken Bayer) , 0,O-dimethyl s-4-oxo-l,2,3,-benzotriazin-3(4H)-ylmethyl phosphorodithioate, is a widely used insecticide. Recently it has been registered for control of a large number of citrus pests including aphids! mites, scales, and brown snails. Extensive residue studies on rhis product have been conducted both in the authors' laboratories and in the Department of Entomology a t the University of California, Riverside: Calif. The latter studies are reported elseivhere ( 7 ) . As cattle feed prepared from citrus waste is an important agricultural commodity, especially along the east coast of the United States, it was decided that a pilot plant study of the effect of processing on Guthion residues in various citrus by-products should be conducted. This study is reported in this paper. The citrus was processed in the pilot plant equipment a t the Citrus Experiment Station. Lake Alfred. ETHIOK
422
AGRICULTURALAND
Fla. The chemical analyses were all performed in the laboratories of Chemagro Corp., Kansas City, Mo.
Materials and Methods Spray Treatments. Pineapple oranges were sprayed with Guthion 25y0 wettable powder a t the rate of 8 ounces active per 100 gallons of spray on December 12, 1961. and January 8, 1962. Control and treated fruit were picked January 22, 1962, and processed January 24. Sixty boxes (90 pounds each) of fruit were collected from both the treated and control plots. Processing Procedure. Processing was carried out according to a standard commercial practice. A flow sheet of the over-all process is given in Figure 1. The washing procedure consisted of a light chlorine rinse, a brushing in a Pacrite Fruit Cleaner G . D. 3A Sudser, a second light chlorine rinse, and a germicidal wash using an 80-pound F O O D CHEMISTRY
pressure spray containing Ultrawet 60
L, trisodium phosphate, and a heavy chlorine concentration. The oranges were then put through water-eliminator rolls during which time they were given another light chlorine rinse. A final light chlorine rinse was made when the samples were on the conveyor. Rotten and split fruit were discarded. Sixty boxes of fruit (approximately 5400 pounds) were used per run, but certain phases of each run were analyzed on a 20-box basis. Juicing was carried out using a Food Machinery Corporation "In-Line Press" with the following settings: three short strainer tubes and two long strainer tubes, 0.040 and 0.090 inch. respectively; restrictor tubes, 7/16 inch; cutters, j / s inch long; beam setting, flush; r.p.m., 50. The finisher used was a Food Machinery Corporation Model 35 with screen openings of 0.020 inch and a head clearance of 0.002-0.006 inch. The crude peel oil emulsion was
Table 1.
Recovery of Guthion and Guthion Oxygen Analog from Oranges and Orange Products P.P.M. Sample
Compound
Cattle Feed (Dry)
Guthion Guthion Guthion oxygen analog Guthion Guthion Guthion Guthion Guthion Guthion oxygen analog Guthion Guthion Guthion oxygen analog Guthion oxygen analog Guthion Guthion Guthion Guthion Guthion Guthion Guthion Guthion Guthion Guthion oxygen analog Guthion Guthion Guthion Guthion oxygen analog
Juice Molasses Oil
Peel Press liquor Pressed peel
Pulp
P.P.M. Control
Added
2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 4.0 4.0 4.0 4.0 2.0 2.0 2.0 2.0
(0.3 C0.3 L0.3
2.0 ~.
(0.3 (0 3
%Recovery
(0.3
C0.3 C0.3 0.3 0.3 0.3 0.7 0.7 0.7 0.7 (0.3 (0.3 (0.3 (0.3
2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 1 .0
82 85 60 102 114 100 99 106 86 80 82 76 75 77 73 93 89 89
95 98 99 96 88 98 97 73 88
(0.3 (0.3 (0.3 (0.3
